Method for detecting carmustat mesylate related substances by adopting high performance liquid chromatography and application

A camostat mesylate and high performance liquid chromatography technology, applied in the field of medicine, can solve the problems of complex impurity spectrum and poor stability of camostat mesylate, and achieve high sensitivity, specificity and simple operation. Effect

Active Publication Date: 2020-10-09
天津泰普制药有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Camostat mesylate has extremely complex impurity profile, poor stability and easy degradation

Method used

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  • Method for detecting carmustat mesylate related substances by adopting high performance liquid chromatography and application
  • Method for detecting carmustat mesylate related substances by adopting high performance liquid chromatography and application
  • Method for detecting carmustat mesylate related substances by adopting high performance liquid chromatography and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 1) Experimental conditions

[0048] Agilent1260-DAD high performance liquid chromatograph;

[0049] Chromatographic column: Waters Xbridge RP18 4.6×150mm 3.5μm;

[0050] Flow rate: 1.0mL / min;

[0051] Column temperature: 35°C;

[0052] Injection volume: 10 μL;

[0053] Sample concentration: 1mg / ml;

[0054] Diluent: 90% acetonitrile aqueous solution;

[0055] Detection wavelength: 230nm and 265nm;

[0056]Mobile phase A: 0.075% (mass fraction) of sodium heptanesulfonate, and 0.1% (volume fraction) of trifluoroacetic acid.

[0057] Mobile Phase B: Acetonitrile

[0058]

[0059] 2) Solution preparation

[0060] Impurity reference substance stock solution: take appropriate amounts of p-hydroxyphenylacetic acid reference substance, intermediate 3 reference substance, intermediate 5 reference substance, impurity C reference substance and impurity J reference substance, weigh them accurately, dissolve with diluent and dilute quantitatively Make a solution containi...

Embodiment 2

[0069] Experimental conditions:

[0070] Agilent1260-DAD high performance liquid chromatograph;

[0071] Chromatographic column: Waters Xbridge RP18 4.6×150mm 3.5μm;

[0072] Flow rate: 1.0mL / min;

[0073] Detection wavelength: 230nm and 265nm;

[0074] Column temperature: 35°C;

[0075] Injection volume: 10 μL;

[0076] Sample concentration: 1mg / ml;

[0077] Diluent: 90% acetonitrile aqueous solution;

[0078] Detection wavelength: 230nm and 265nm;

[0079] Mobile phase A: 0.075% (mass fraction) of sodium heptanesulfonate, and 0.05% (volume fraction) of trifluoroacetic acid.

[0080] Mobile Phase B: Acetonitrile

[0081]

[0082] 2) Solution preparation

[0083] Impurity reference substance stock solution: take appropriate amounts of p-hydroxyphenylacetic acid reference substance, intermediate 3 reference substance, intermediate 5 reference substance, impurity C reference substance and impurity J reference substance, weigh them accurately, dissolve with diluent an...

Embodiment 3

[0092] Experimental conditions:

[0093] Agilent1260-DAD high performance liquid chromatograph;

[0094] Chromatographic column: Waters Xbridge RP18 4.6×150mm 3.5μm;

[0095] Flow rate: 0.8mL / min;

[0096] Detection wavelength: 230nm and 265nm;

[0097] Column temperature: 35°C;

[0098] Injection volume: 10 μL;

[0099] Sample concentration: 1mg / ml;

[0100] Diluent: 90% acetonitrile aqueous solution;

[0101] Detection wavelength: 230nm and 265nm;

[0102] Mobile phase A: 0.075% (mass fraction) of sodium heptanesulfonate, and 0.10% (volume fraction) of trifluoroacetic acid.

[0103] Mobile Phase B: Acetonitrile

[0104]

[0105] 2) Solution preparation

[0106] Impurity reference substance stock solution: take appropriate amounts of p-hydroxyphenylacetic acid reference substance, intermediate 3 reference substance, intermediate 5 reference substance, impurity C reference substance and impurity J reference substance, weigh them accurately, dissolve with diluent an...

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Abstract

The invention provides a method for detecting carmustat mesylate related substances by adopting high performance liquid chromatography. A chromatographic column is an octadecylsilane chemically bondedsilica chromatographic column, and a mobile phase A is a mixed solution of sodium heptanesulfonate and trifluoroacetic acid; a mobile phase B is any one of acetonitrile, methanol, ethanol and tetrahydrofuran or a mixed solution of two of acetonitrile, methanol, ethanol and tetrahydrofuran; a diluent is pure water or a mixed solution of pure water and any one or two of methanol, acetonitrile, ethanol and tetrahydrofuran. The method can be applied to determination of carmustat mesylate related substances and determination of residual quantity in drugs using 4-dimethylaminopyridine as a catalystand N, N-dimethylformamide as a refining solvent in a synthesis process.

Description

technical field [0001] The invention belongs to the technical field of medicine, and specifically provides a method for detecting related substances of camostat mesylate by using high-performance liquid chromatography, and the detection method adopts liquid chromatography. Background technique [0002] Camostat mesilate (English name: Camostat Mesilate) chemical name becomes 2-(dimethylamino)-2-oxoethyl 4-(4-guanidinobenzoyloxy)phenylacetate A Sulfonate, molecular formula C 20 h 22 N 4 o 5 •CH 3 SO 3 H, molecular weight 494.52, CAS accession number: 59721-29-8. Its structure is as shown in formula I: [0003] [0004] Camostat mesylate is a non-peptide protein inhibitor. After oral administration, camostat mesylate quickly acts on the body's kinin production system, fibrinolytic system, coagulation system and complement system, inhibiting the abnormal hyperactivity of enzyme activities in these systems, thereby controlling the symptoms of chronic pancreatitis and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/74G01N30/06G01N30/04G01N30/88
CPCG01N30/02G01N30/34G01N30/74G01N30/06G01N30/04G01N30/88G01N2030/047G01N2030/884G01N2030/8872
Inventor 张慕军石涛雷勇胜邓瑶崔轶达丁文宇刘桂霞史可吟
Owner 天津泰普制药有限公司
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